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citizen of the United States, and a resident of Montclair, in the county of Essex and. I State of New Jersey, have invented certain new and useful Improvements in'-Binding Agents, of-whrch the following is a specification.

This invention relates to a binding material prepared from waste sulfite cellulose liquor and contains matter derived from my copending applications Serial No. 779,516 filed July 17, 1913, and 757,801 (now Patent 1,246,805).

M invention specifically relates to the prodiiction of a binder consisting of, or containing, waste sulfite $|lulose liquor solids in the form 0 a pow er or granu ar ragmentagy material in such a condition as to be res i U so that t e material may he reduced or dissolved in to make a solution of the desired density or viscosity. Waste sulfite cellulose liquor when dried to a solid material according to any of the old processes, and without proper precautions not infrequently exhibits a tendency to under 0 undesirable changes which render it inso uble or prone to become insoluble in storage or to unduly absorb moisture, becoming sticky, lumpy and compacted or otherwise modified due to atmoLsiplieric or aging influences.

y invention is particularly directed to the production of a stable dry composition or product comprisin sulfite cellulwe waste liquor solids, suc binder bein sufficiently stable so that it may be pac ed in barrels, such as flour barrels; which, of course, are more or less pervious to the air and in this condition the product may be shipped or stored and thus exposed to the air for weeks or even months without becommg insoluble to any material extent and in the preferred form of the invention with .advantageous qualities as regards relative resistance to moisture which would render it hightly useful for shipment in humidclimates. The sulfite liquor roduct may be pre ared by evaporating 0 li nor in an aci state and to this end it is esirableto reduce the acidity of the liquor at the beginning. after, or during the course of the concentration. This may be brought about by the addition of a quantity of alkali, lime or substantially soluble in water a STATES PATENT OFFICE.

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1,311,216. menswear Patented Jnly 29,1919. Io mm.f j unuumrmnmr. aamlaimra' W2 1 Toallwlwmitma concern: be i eficient for the purpose but soda or Be it known tliat I. Casinos Ems, a mg other elk. he may be used if desired, such W5 mg added in such amount as to re duce the acidity, more or less, but preferably to about one-half (and preferably to not much below this amount) the original normal acidity, producing what may be termed, a semi-acid material.

In the d or concentration of ordinary unneutrali xda or partly neutralized sulte waste liquor, volatile acids contained in the liquor, such as dissolved sulfur dioxid, will normally be vaporized and accordingly removed from the liquor. In referring herein to the acidity of sulfite waste liquor, it is accordingly advisable to distinguish between that rtion of the acidity of the liqiior, which is caused by the presence of nonvolatile substances (referred to as fixed acidity), and that portion of the acidity which is caused by the resence of dissolved SO and other relative y volatile substances which will be normally vaporized, and hence removed from the liquor during concentration and evaporation (referred to as volatileacidity Instead of concentrating to a syrupy body of say 30 B, I may carry the concentration much farther, removin preferably almost the entire conte mj'i ater that is fZi'say, dehydrating ihe material suiiiciently at least to produce a solid form. This dehydration may be carried out in the presence of oxysmall quantities ordinarily being sufcient so as to produce oxidation of t e sulfite liquor during the drying operation. It

is usually customary to concentrate sulfite liquor in vacuum pans in the absence of air but in the present casein the preferred form of ,the invention a regulated degree of oxidation is desirably produced by drying o r desiccating in thergresence of small quantities of oxygen. is for example, may be carried out by drying in an atmosphere of reduced oky n content. Whil'T may'a'se' aucli semi-acid material as aforesaid, I do not w o 1 'm If strictly to such a product but may use various other forms of the sulfite liquor suitable for the present purpose.

As stated in Serial No. 757,301 the sulfite li n01 mav'be dried in an atomizlng system which yields the solids thereof in a pulverulent condition, or in other cases the liquor may be dried to a solid and ground to a powder. Preferably I carry out the drymg in part at least by atomization, in which case contact with oxygen contained in the drying 5 gases produces a slight degree of oxidation which may be referred to as a quick aging and 'ves in a cheap and effective manner valutfiile properties, such as stability to the product; such product constitutes one form 10 of material em raced within the present invention. In its preferred form the product is a fine ranular or pulverulent material and is satlsfactorily soluble in water. Although the semi-acid sli htl -oxidized material is origima an me in the dry form when made in accordance with the preferred procedure hereof, such product as the property of becoming more or less insoluble from protracted exposure to air and moisture so that it ma be used as a binder for road beds and roa surfaces or for making briquets with coal, iron ore, sawdust, minera fillers, talc, ma nesife, sand, crushed 25 roc er, as'b'e's't os culm and Elie like. It. may also be used as a core compound and for other purposes for which a bindin sub; stance is desired. Likewise it may applied as a tanning agent and such product, as the advantage of ease of shipment as a dry powder in contrast to the difiiculties of shipping and handling syrup sulfite liquors.

Fillers such as talc, kiesel hr fuller -t allfiongeptgated..liquog so as to form a hiicleus dilrln W n enda'lli wei g n t: the. samenessmyem sired. Thus the liquor may be partially concentrated in vacuum pans or any other suitable concentratin a paratus, a filling material such as kiese gu r added and the evaporation continued in heated air containing a reduced content of oxygen so as to roduce the slightly oxidized product an bring about the evaporation of the moisture to yield the dry material. This thus involves a two stage operation of drying which is advantageous under some conditions. Of course, the dryin may be carried out in a similar manner without the addition of any I filling material.

material may be; ad; so a so iiim 16a The sulfite li u riiixedwith Sll lc af o ms 5 or 10% or so of si ligat e of so ,may be mnded'wmsuquor prior to us concentra tron. It is better to mix the d pulverized sulfite li uor binder with dry si l lcajgpj p dg in {he I or 'm' of a powder using various proportions of the latter, to ordinarily being useful, thus afi'ording a mixture of the pulverulent sulfite liquor solids and silicate of soda. 65 In other cases (as stated in Serial No.

239,882) a quantity of etroleum oil may be added to the binding agent, Ill 0 15-% of petroleum oil, such as as haltic Oll be ng useful to aid in waterpr g e material. Under some conditions only 3 to 5% of oil, or 1% or so of calcium stearite gives the desired yvaterproo ng e co he petroleum oil, may for example, be added to the liquor after the latter has been concentrated to a thick syrup when the product may be brought to dryness and if evaporated under conditions giving solid masses of material this may be pulverized to form a powder or if the product is obtained by atomization a granular or finely-divided pulverulent material is directly obtained.

My invention yields a product of a very desirable character for shipping purposes and for ready solubility in water or other aqueous medium and the prefeTr'e'd form as stated is particularly advantageous in view of a desirable tendency to resist the action of atmospheric moisture to a considerable degree so that when stored and packed in containers which allow access of the air, the

product is not readily affected to an undesirable extent but answers requirements in this respect in an advantageous manner. A product prepared by the drying by atomization of acid sulfite cellulose waste li nor to yield a PI veru en proc no 0 1s sta lccharacter in which slight oxidation has taken place during drying due to contact with the heated atomizing and drying gases containing less oxygen than is normal in ordlnary air is partlcularly recommended.

Cross reference is here made to my copending cases as follows:

779,516, filed July 17, 1913, (renewed June 13, 1918, Serial No. 239,882) for drying sulfite waste li uor, preferably after the neutralization of a material portion, but not all of its original acidity, for example, by the neutralization of about half of the acidity and then drying the roduct, and this wit or without the addition of silicate of soda or other named materials for the production of specific effects. I also claim therein, products produced by such treatment, 167,332, filed May 8, 1917, for drying and grinding acid sulfite waste liquor, and prod uct thereof, 168,275, filed May 12, 1917, for a solution of dried acid sulfite waste liquor solids, 188,860 filed August 27, 1917, for a particular mode of atomizing, drying and oxidizing the sulfite waste liquor, to oxidize the least stable portion of the solid contents thereof. This case includes claims to the specific process herein described.

Cross reference is also made to shaped products and to the production thereof by the use of the product claimed herein in my copending cases as follows: 161,111, filed April 30, 1917; 176,280, filed June 22, 1917; and 186,481, filed August 16, 1917, and to a soluble, relatively stab mixture of the present product with lime or equivalents claimed in 201,807 filed November 13, 191%.

What I claim is L'Sulfite liquor solids, of an acid character, dried by atomization.

2. Snlfite liquor solids, of an acid character but having an acidity materially less than that of the raw liquor from which said solids were produced, and being dried by atomization. 3. As a binding agent, acid sulfite cellulose waste liquor solids in ulverulent form and slightly oxidized con ition, said product being water-soluble and bein substantially resistant to atmospheric in uences for an indefinite period. I

4. As a bindin agent, sulfite cellulose waste li uor soli s in a pulverulent form and slig tly oxidized condition, soluble in water.

5. As a binding agent, atomized sulfite cellulose waste liquor solids of an acid character, in a pulverulent form and oxidized condition.

6. A binder in a powder form comprising slightly oxidized waste cellulose sulfite liquor solids dried by atomization, said powder bein of an acid character, and when package in containers pervious to air bemg re atively stable in storage, and having the property when mixed with bulkin material of becoming substantially insolu 1e on protracted exposure to air and moisture.

7. Apulverulent form of acid waste sulfite cellulose liquor solids of partially reduced acidity, in a sli htly oxidized, watere condition.

8. A pulverulent form of waste sulfite celflopica at this patent may be obtained for the cents each, by droning the Washington, D. 0."

,lulose liquor solids in an oxidized but watersoluble condition.

9. Waste sulfite cellulose liquor acid solids d iied by atomization and admixed .with an 01 10. As a binding agent atomized dried sulfite cellulose waste liquor solids in a slightly oxidized acid condition, admixed with a waterproofing agent.

11. As a briqueting agent or binder, atomized oxidized acid sulfite cellulose Waste liquor solids in a. dry pulverulent form, so uble in water and relatively stable.

12. As a briqueting agent or hinder, atomized oxidized sulfite cellulose waste liquor acid solids in a dry water-soluble form.

13. A binder composition comprising solid oxidized constituents of waste sulfite cellulose liquor which has its normal acidity reduced about one-half.

14. As a binding agent, a finely divided, slightly oxidized, air-stable, substantially non-hygroscopic, solid, dry product, containing $111 to cellulose wasteliquor solids in a somewhat acid state.

15. As a binding agent, atomized sulfite cellulose waste liquor solids in a dry pulverulent form, acid in reaction.

16. As a binding agent, atomized sulfite cellulose waste liquor solids containin a substantial proportion but substantially less than all of the acidity of normal sulfite waste liquor, said materia existing as a substantially dry roduct.

17. As ainding agent, pulverulent atomized sulfite li uor solids, slightly oxidized, but readily so uble and air-stable.

CARLETON ELLIS.

Commissioner of Patents, 

